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In order to obtain diamond-like carbon (DLC) thin films with improved mechanical, tribological, thermal and corrosion properties for practical applications, the structure and properties of various DLC thin films including hydrogen-free DLC, hydrogenated DLC, and DLC-MoS2 composites synthesized under different conditions were investigated in this thesis. The research methodologies and the main results are summarized in following paragraphs. Hydrogen-free DLC thin films were synthesized by biased target ion beam deposition (BTIBD) method, while hydrogenated DLC thin films were deposited by ion beam deposition technique using a Kaufman-type ion source and an end-Hall ion source. DLC-MoS2 composite thin films were also synthesized using BTIBD technique in which MoS2 was produced by sputtering a MoS2 target while DLC was simultaneously deposited by ion beam deposition. The influence of processing parameters on the bonding structure, morphology and properties of the deposited films was investigated using atomic force microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, synchrotron based near edge X-ray absorption fine structure spectroscopy, X-ray diffraction, scanning electron microscopy, nanoindentation, ball-on-disk and corrosion testing. Finally, the influence of annealing temperature on the structure and properties of pure DLC and DLC-MoS2 composite films in ambient air and low pressure environments was studied. In the case of BTIBD method, hydrogen-free DLC thin films with exceptionally high smoothness and low friction coefficient were prepared by biased target sputtering of graphite target without additional ion bombardment either by negative bias of substrate or assisting ion source. For ion beam deposition technique with Kaufman ion source, the DLC thin films synthesized at ion energies of 300 eV showed the highest sp3 content and optimum properties. Regarding end-Hall ion source, the best properties achieved in DLC films synthesized at ion energies of 100 eV. Comparing with pure DLC and pure MoS2 films, the DLC-MoS2 films deposited at low biasing voltages showed better tribological properties including lower coefficient of friction and wear coefficient in ambient air environment. Also, comparing with pure DLC films, the DLC-MoS2 thin films showed a slower rate of graphitization and higher structure stability throughout the range of annealing temperatures, indicating a relatively higher thermal stability.

This thesis deals with the study of the effect of the constituents of the model synovial fluid on the frictional properties of articular cartilage. The influence of constituents, concentration, speed and load is observed. Experiments were performed on a commercial tribometer at configuration pin-on-plate. Several types of lubricants containing synovial fluid constituents have been selected for the experiments. Lubricants were prepared at two concentrations, the concentration of healthy individuals and at a concentration typical of for osteoarthritic patients. Speeds 5 and 10 mm/s and 5 and 10 N loads were used for all experiments. It is shown that when using only lubricant containing proteins, no difference in the coefficient of friction is observed and the effect of concentration is also not observed. The addition of hyaluronic acid has a synergistic effect with -globulin, however in the case of lubricants containing albumin, the effect is opposite. After the addition of phospholipids, no significant effect on friction is observed in -globulin containing lubricants. No significant effect of the composition and concentration of the lubricants is observed with the load change.

Hydrogen is a clean and sustainable form of carrier of energy that can be used in mobile and stationary applications. At present hydrogen is produced mostly from fossil sources. Solar photoelectrochemical processes are being developed for hydrogen production. Storing hydrogen can be done in three main ways: in compressed form, liquid form and by chemical bonding. Near term spaceport operations are one of the prominent applications for usage of large quantities of liquid hydrogen as a cryogenic propellant. Efficient storage and transfer of liquid hydrogen is essential for reducing the launch costs. A Two Stage Reverse Turbo Brayton Cycle (RTBC) CryoCooler is being developed at University of Central Florida. The cryocooler will be used for storage and transport of hydrogen in spaceport and space vehicle application. One part in development of the cryocooler is to reduce the friction and wear between mating parts thus increasing its efficiency. Tribological coatings having extremely high hardness, ultra-low coefficient of friction, and high durability at temperatures lower than 60 K are being developed to reduce friction and wear between the mating parts of the cryocooler thus improving its efficiency. Nitrides of high-melting-point metals (e.g. TiN, ZrN) and diamond-like-carbon (DLC) are potential candidates for cryogenic applications as these coatings have shown good friction behavior and wear resistance at cryogenic temperatures. These coatings are known to have coefficient of friction less than 0.1 at room temperature. However, cryogenic environment leads to increase in the coefficient of friction. It is expected that a composite consisting of a base layer of a hard coating covered with layer having an ultra-low coefficient of friction would provide better performance. Extremely hard and extremely low friction coatings of titanium nitride, molybdenum disulphide, TiN/MoS2 bilayer coatings, DLC and DLC/MoS2 bilayer coatings have been chosen for this application. TiN film was deposited by reactive DC magnetron sputtering system from a titanium target and MoS2 film was deposited by RF magnetron sputtering using a MoS2 target. Microwave assisted chemical vapor deposition (MWCVD) technique was used for preparation of DLC coatings. These composite coatings contain a solid lubricating phase and a hard ceramic matrix phase as distinctly segregated phases. These are envisioned as having the desired combination of lubricity and structural integrity. Extremely hard coatings of TiN and DLC were chosen to provide good wear resistance and MoS2 was chosen as the lubricating phase as it provides excellent solid lubricating properties due to its lamellar crystal structure. This thesis presents preparation; characterization (SEM and XRD), microhardness and tribological measurements carried out on TiN and TiN/MoS2 coatings on aluminum and glass substrate at room temperature. It also presents initial development in preparation of DLC coatings.

Le chrome dur, utilisé comme revêtement de tige d’actionneurs hydrauliques linéaires, a été interdit pour risque sanitaire (directive européenne REACH). A cet effet, un revêtement de WS2 a été sélectionné par Safran Landing Systems pour substituer le chrome dur comme revêtement de tige de piston de frein hydraulique. La démarche de sélection utilisée, est limitée par son incapacité à expliquer les performances observées et démontre le besoin d’une démarche de sélection d’autant plus appropriée que la notion d’étanchéité des actionneurs hydrauliques linéaires est « floue ». Comme, la tribologie n’a pas vocation à caractériser les revêtements de surface, parce que son plus petit objet d’étude est un triplet tribologique, cette étude propose l’évaluation de la compatibilité tribologique du revêtement de WS2, avec la fonction d’étanchéité. La démarche utilisée montre que l’étanchéité est régie, par un critère en pression, et par une vérification des caractéristiques tribologiques du système tige/joints requises pour la réalisation de l’étanchéité ; ce qui nécessite un piston hydraulique instrumenté. L’absence de ce piston est compensée par une « caractérisation tribologique approchée » du contact tige/joints, qui associe les expertises tribologiques de pistons hydrauliques d’essais de qualification, appuyées par un modèle éléments finis (EF) du piston hydraulique d’une part, et les résultats d’un essai de frottement piste/joints, conçus à cet effet à l’aide d’un modèle EF d’autre part. Les résultats montrent que le système tige/joints présente de bonnes caractéristiques tribologiques pour le facteur de frottement et l’usure, alors que la localisation de l’accommodation de vitesses dans le cas du contact tige/joint d’étanchéité, accélère le débit source du revêtement et limite sa durée de vie. Enfin, cette thèse comble un vide méthodologique en proposant, une démarche de sélection d’un revêtement pour une application tribologique, et une démarche de triboconception d’un actionneur hydraulique linéaire dans le cas d’un fonctionnement quasi-statique. / Hard chromium used as rod coating in linear hydraulic actuators has been forbidden by the European Directive REACH. In this situation, a WS2 coating has been selected by Safran Landing Systems to replace the hard chromium coating on rod pistons actuators of landing gear braking systems. The selection method was unable to explain the observed performance, and shows the lack of an appropriate methodology for the rod coating selection, mainly because the sealing concept is rather vague. Since tribology is not intended to characterize surface coatings, because its smallest object of study is a tribological triplet, this study proposes the evaluation of the tribological compatibility of the WS2 coating with the sealing function of the hydraulic piston. The adopted approach shows that the sealing performance is governed by a rod/seal contact pressure criterion and by the verification of the tribological characteristics of the rod/seal contact required to achieve a sealing performance. This tribological characterization requires an instrumented hydraulic piston. The absence of this piston is compensated by an "approximate tribological characterization" of the rod/seal contact, which combines the tribological expert analysis of hydraulic pistons of qualification tests, supported by a finite elements model (FE) of the hydraulic piston, and the results of a plate rod/seal friction test, designed for this purpose using another FE model. The results show that the rod/seal contact exhibits good tribological characteristics for the friction factor and wear, whereas the location of the velocity accommodation in the case of the rod/anti-extrusion seal contact accelerates the 3rd body generation of the coating and limits its life expectancy. Finally, this thesis fills a methodological lack by proposing a method of selecting a coating for a tribological application and a triboconception method of a linear hydraulic actuator in the case of quasi-static operating conditions.

The thesis comprises the two parts in each chapter: the first part focuses on the development and characterization of polyimide (PI) based composite coatings on a steel substrate. In order to improve the tribological performance of polyimide coatings, the fillers i.e. multi-walled carbon nanotubes (MWCNTs) and Graphene (GP) were added into PI and conducted friction test at elevated temperatures ranging from room temperature (RT) to 200°C. Also, the influence of fillers (MWCNTs and GP) materials into PI coatings surface, mechanical and tribological properties of polyimide composites coatings are measured. The addition of MWCNTs and GP reduces the friction coefficient as well as wear volume at elevated temperatures 50°C, 100°C and sometimes at 150°C. These temperatures play a vital role to form a lubrication layer in the contact interfaces at certain load and operating conditions. In these cases, three weight percentage (3wt%) of MWCNTs and GP into polyimide composites showed low friction and high wear-resistant as compared to other PI composites. Besides, by adding these two fillers into pure PI improved the mechanical properties such as micro-hardness and nanoindentation. The scanning electron microscope (SEM) was used to observe the wear mechanism of the composite coatings worn surfaces. The consequences expose that the fatigue wear mechanisms were predominant in the worn surfaces. Moreover, the thermal study of the polyimide composite coatings was conducted using thermal gravimetric (TG) to analyze the behavior of composite coatings at high temperatures. The results showed that the PI coatings with MWCNTs and GP have high thermal stability at 60% sample residue. In the second part-an epoxy coatings with filler materials e.g. hexagonal boron nitride (h-BN) and expanded graphite (EG) were made and conducted their tribological i.e. friction coefficient and wear performance. Also the perfect mixing ratio 4:1 (80 wt% base epoxy matrix and 20 wt% curing agent) was determined on the basis of stoichiometric ratio to cure the epoxy accurately. Therefore, seven samples with a various weight percentage (wt%) were prepared i.e. pure epoxy, epoxy with 5wt%, 10wt%, 15wt% of h-BN and EG. All the prepared samples ran at two different loading 2 N and 4 N conditions with 5 Hz frequency, 300 rpm and 30 minutes duration. The epoxy with h-BN showed low friction as compared to EG where EG has better wear-resistant behavior than h-BN.

Os principais mecanismos de desgaste, presentes em discos de freio ventilados automotivos, foram determinados utilizando ensaios de bancada em dinamometro inercial. Foram medidas a temperatura, rugosidade, taxa de desgaste, tensões residuais, coeficiente de atrito e desempenho de frenagem. Foi analisado o tribocontato através de técnicas de microscopia eletrônica e ótica. / The main mechanims of wear, present in ventilated brake disc had been determined, when submited to the braking test in inertial dynamometric simulator. Were measured wear taxes, temperature, residual stresses, friction coeficient, topographic of relief and analised their tribographics.

Bulk forming and cutting are widely used to shape metals in industrial production. Bulk forming is characterized by large strains, extensive plastic deformation and large surface expansions. Cutting is characterized by high speeds, high pressures and high temperatures. The prevailing conditions during these processes lead to transfer of work material to tools. In bulk forming this is a significant problem. The transferred work material is hardened and becomes harder than the work material, causing galling. This leads to high friction and high forming forces, bad surface finish of the formed products and significant difficulties to produce complicated geometries. In cutting, transfer of work material can be desired for protection of the tool surface. However, the transfer film has to be of the correct type to provide a stable and predictive behaviour during operation. In this thesis the influence from tool material and surface treatment on work material transfer has been studied for both applications, with the use of simplified laboratory test methods followed by extensive surface studies. Both the tendency to, appearance of and chemical composition of work material transfer is evaluated. The results are compared with real industrial examples, to ensure that the correct mechanisms are mimicked. In forming, the problems arise when poor lubrication prevails, due to high forming forces or large surface expansions. The transfer of work material can then be avoided with the use of a galling resistant coating, offering low adhesion. However, the coating has to be as smooth as possible, to avoid activation of the work material and subsequent transfer. In cutting, the desired transfer film can be obtained by choosing the correct cutting parameters. The geometry and material of the fabricated component is often predetermined, setting the general cutting conditions, but the cutting speed influences the formation of the transfer film. Too low speed or too high speed leads to an unstable cutting process and poor surface finish of the piece. The speed intervals for each mechanism are partly determined by the tool material and thus by the tool coating.

This research investigated the tribological performance of a composite material, formed from an ultra high molecular weight polyethylene (UHMWPE) matrix and quasicrystalline Al-Cu-Fe alloy powders. An evaluation was conducted for the microstructure, material properties, and tribological performance of quasicrystalline materials formed from Al-Cu-Fe alloys. Arc melting was used as the fabrication technique for these alloys, and some samples were additionally heat treated in an argon environment. Vickers microhardness testing was done to make comparisons to wear rate behavior of the various alloys. Tribological studies were conducted using a linear pinon- desk configuration to evaluate friction and wear. Research indicated the annealed samples of Al-Cu-Fe that formed icosahedral quasicrystalline phases, where the quasicrystalline phase was most dominant of the observed alloys, displayed the greatest wear resistance and hardness. Abrasive wear was observed in each of the samples, as the brittle, hard nature of the quasicrystalline phase would not allow for the ductile adhesion. The addition of small amounts of Al-Cu-Fe quasicrystalline particles, crushed and pulverized from the arc-melted ingots, reduced the coefficient of friction and wear rate of UHMWPE, when added to the polymer.

As vantagens relacionadas à utilização de revestimentos duros depositados via processos PAPVD (Plasma Assisted Physical Vapor Deposition) são bem conhecidas e dadas por suas propriedades. As principais propriedades destes filmes são a capacidade de não incrementar significativamente a rugosidade dos substratos em que são depositados, sua alta dureza conferindo alta resistência ao desgaste, baixa reatividade quando se trata de revestimentos de compostos cerâmicos e capacidade de reduzir o coeficiente de atrito de pares tribológicos inseridos em diversos meios. A nitretação a plasma de substratos antes da aplicação de um revestimento faz com que outros benefícios possam ser encontrados, dentre eles destacam-se o aumento da capacidade de sustentação de carga do substrato e a criação de uma região que propicia um gradiente de propriedades entre o substrato e o revestimento. Desta forma é caracterizado o tratamento dúplex, o qual consiste em um substrato nitretado seguido da aplicação de um revestimento. Através do processo de nitretação a plasma, camadas de difusão foram formadas em amostras de geometria cilíndrica do aço DIN X100CrMoV8-1-1, industrialmente utilizado para construção de ferramentas para operações de corte e estampagem. Duas profundidades distintas de camada de difusão foram formadas. O revestimento escolhido para este estudo foi o TiCN (carbonitreto de titânio), produzido industrialmente e disponível no mercado brasileiro. As técnicas de caracterização foram utilizadas para medir a rugosidade, a dureza, os perfis de composição química, as fases formadas, as tensões residuais e a adesão dos revestimentos. Após esta caracterização inicial, foram feitos ensaios utilizando a técnica de esfera-sobre-disco em amostras e de DST (Dobramento sob Tensão) em pinos com geometria específica com o objetivo de se avaliar o comportamento tribológico dos tratamentos dúplex desenvolvidos. / The advantages related to the utilization of hard thin films deposited on tools and components via PAPVD (Plasma Assisted Physical Vapor Deposition) are well known and given by their properties. The main properties of these coatings are their capacity to avoid significant roughness increase of the coated substrates, high hardness which provides high wear resistance, low reactivity in the case of ceramic coatings and the possibility to provide very low friction coefficient. The thin films associated with plasma nitriding (the so called duplex treatments) applied to the substrates can bring much more benefits. The coating load bearing capacity can be increased by the presence of the diffusion zone on the substrate that allows a gradient of mechanical properties from the coating to the core of the material. In this work, by plasma nitriding process, two distinct depths of diffusion layer were developed in samples and pins manufactured out of the DIN X100CrMoV8-1-1 steel. This steel grade is commonly used to manufacture tools for cutting and stamping operations. Following a previous work the chosen coating for this study was a graded TiCN (titanium carbonitride). The samples were characterized by several different techniques in order to access surface roughness, chemical composition profiles, present phases, residual stresses, hardness and adhesion of the obtained nitrided layer and coatings. After this initial characterization, tests were performed using a pin-on-disc apparatus and BUT (Bending under tension test) with the aim to evaluate the tribological behavior of the developed duplex treatment for for sheet metal forming application.